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Copyright of Shipin Kexue/ Food Science is the property of Food Science Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Shipin Kexue/ Food Science is the property of Food Science Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

The growing prevalence of pharmaceutical compounds in the environment raises significant concerns due to their potential impacts on ecological and human health. This present manuscript focuses on the methods used to extract and determine these pharmaceuticals in water samples. It provides a comprehensive analysis of the extraction techniques and analytical approaches employed for the identification and quantification of pharmaceuticals in environmental water. Due to their chemical properties and widespread use, pharmaceuticals persist in the environment and contaminate water bodies, soil, and sediments. The presence of pharmaceuticals in the aquatic environment has been linked to several adverse effects on aquatic organisms, including the disruption of physiological processes and reproductive impairment. Furthermore, pharmaceuticals in the environment can affect human health through food and drinking water contamination and contribute to antibiotic resistance. The analysis of pharmaceutical contaminants in water samples presents several challenges due to the complex matrix and low concentrations of target substances. Various sample preparation techniques and protocols, including solid-phase extraction (more than 76% of the studied literature) and QuEChERS (quick, easy, cheap, effective, rugged, and safe), coupled with liquid chromatography–tandem-mass spectrometry, are commonly used for their determination. These methods offer high sensitivity, selectivity, and efficiency in identifying and quantifying pharmaceuticals in environmental samples. It is, therefore, essential that ongoing research is conducted in order to develop more efficient analytical methods and mitigation strategies to address pharmaceutical contamination in the environmental water effectively. It is also crucial that increased awareness and regulatory measures are put in place in order to minimize the environmental and human health risks associated with pharmaceutical pollutants. [ABSTRACT FROM AUTHOR]

Free fatty acids (FFAs) serve as crucial analytical markers in oils, fats, and food, reflecting food safety through their content variations. However, the analysis of FFAs in food samples is constrained by potential interferences from other acidic components in the sample matrix during sample processing, resulting in distorted analytical outcomes and introducing positive bias. The established method was also validated in terms of linearity, limits of detection (LOD) and quantification (LOQ), and matrix effect. It was proved to be linear (R2 > 0.99), with lower LODs of 0.108–0.564 μg/mL, and lower LOQs of 0.258–1.541 μg/mL for all FFAs. Overall, the simple, rapid, and cost-effective method developed in this study provides a potential application for the extraction and enrichment of FFAs in complex sample matrices, including edible oils, fatty foods, and high-content biological samples. [ABSTRACT FROM AUTHOR]

Wheat is considered as staple food source for 40% of the population worldwide. Yet, the yield and quality can be compromised by fungal diseases, which are also responsible for mycotoxins presence at wheat seeds and originating foodstuff. In this context, the tackling of this problem by developing regulatory limits and standards have induced the development of various methods for sampling, extraction, identification and quantification of mycotoxins in food samples. This review addresses the comparison of the technical and cost efficiency of methods for the extraction and qualitative- quantitative analysis of mycotoxins from whole wheat flour. Methods of extraction such as the Solvent Extraction method, the Liquid Liquid Extraction, the Solid Liquid Extraction, the Solid Phase Extraction, the Immuno-Affinity Columns, the QuEChERS, and the use of absorbent nanomaterials such as graphene oxide and multi-walled carbon nanotubes in extraction procedures, are described in principle, technical details are presented, and examples of reported use are given. Methods of mycotoxin analysis such as Immunological Assays (LFIA, ELISA, FPIA), the Sensor-based (Surface Plasmon Resonance Sensor, Piezoelectric Sensors, Electrochemical Sensors, Colorimetric Sensors), and Chromatographic Techniques (TLC, GC, HPLC, HPLC-FLD, LC-MS/MS, UPLC-MS/MS, UHPLC-MS/MS, UFLC-MS/MS) are reviewed. To compare their efficiency, main advantages and disadvantages, the ongoing improvements, as well as the validation parameters (linearity, recovery range, RSDr range, RSDR %, LOQ range, and cut off) are summarized, and pairing of extraction to analysis methods for specific mycotoxins is provided. It was evidenced that none of methods already in use is capable of analyzing all mycotoxin categories at once, because of their chemical characteristics (volatile/non-volatile, co-elution, UV absorption, fluorescence) versus methods restrictions (matrix interferences, cross-reactivity of antibodies, selectivity and reproducibility of data, need for derivatization, etc). Also, depending on the purpose of the analysis (research or screening as part of legal requirements), to date the immunological methods are only suitable for validated matrices, biosensors can be used for routine screening, and that GC-MS and HPLC-based methods fulfill the legal requirements. In conclusion, while the selectivity and accuracy of methods for mycotoxin detection is being improved rapidly (those sensor-based thanks to the use of nanoparticles, nanomaterials, aptasensors, etc., and the chromatographic techniques coupled with mass spectrometry offer a higher selectivity and sensitivity, low detection limits, maintained resolution performance), and the duration of the analysis, the cost, and the need for highly-skilled staff go in favor of rapid methods (immunological and sensors-based), it is the capacity to fulfill legal requirements, which will determine the trend and their future success in the market. [ABSTRACT FROM AUTHOR]

This research describes an easy, rapid, and inexpensive magnetic solid-phase extraction (MSPE) approach employing Fe3O4 magnetic nanoparticles modified with cetylpyridinium chloride (Fe3O4@CPC/MNPs) for extracting amoxicillin (AMX) and doxycycline (DOX) after derivatization with 4-chloroaniline as a color reagent. The azo-coupling of AMX and DOX with the color reagent in the alkaline medium caused yellow and yellow-orange azo dyes with maximum absorption wavelengths of 435 and 438 nm, respectively. The UV–Vis spectroscopy was utilized to determine the target analyte after the extraction procedure. Good linearities (R2 > 0.99) in the concentration ranges of 0.03–4.50 and 0.05–6.00 µg/mL were obtained for AMX and DOX, respectively. The experimental detection limits of AMX and DOX were obtained as 0.01 and 0.02 µg/mL, respectively. The developed approach was effectively applied to pre-concentrate and quantify AMX and DOX in environmental water and urine samples. [ABSTRACT FROM AUTHOR]

Accurate measurement of serum glycocholic acid (GCA) is crucial for evaluating the activity of chronic hepatitis. Moreover, GCA is a novel identified biomarker for hepatocellular carcinoma. Although some laboratories have used the liquid chromatography-tandem mass spectrometry (LC–MS/MS) method to measure GCA in recent years, the problem of potential interference of GCA analogues has not been solved well yet. Neither reference measurement procedures nor reference materials for GCA have been listed in the Joint Committee for Traceability in Laboratory Medicine (JCTLM) database. For standardization of GCA, it is urgent to establish a candidate measurement procedure for GCA. In this study, a candidate reference measurement procedure for the quantification of GCA in human serum based on isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC–MS/MS) by a two-step sample pretreatment of protein precipitation and MAX solid-phase extraction was developed and validated. GCA can be completely separated from its structural analogues with gradient elution in 9 min compared with short time gradients published in previous literature by Huang's group. Method validation indicated perfect quantitation precision with intra-day and inter-day values that were ≤1.30% and ≤1.80%, respectively. The method showed excellent linearity with high regression coefficients (R2 > 0.999) over a range of 0.92 ng/g–38.38 μg/g and perfect recoveries at three spiked levels (99.87–100.43%). No interference, matrix effect, and carryover were observed. Moreover, the cRMP was successfully applied to measure GCA in serum samples and compared with two immunoassays in a clinical laboratory. As a candidate reference method, this method can promote a GCA standardization program. [ABSTRACT FROM AUTHOR]

Background: Wastewater can contain a complex mixture of organic micropollutants, with both chemical analysis and effect-based methods needed to identify relevant micropollutants and detect mixture effects. Solid-phase extraction (SPE) is commonly used to enrich micropollutants prior to analysis. While the recovery and stability of individual micropollutants by SPE has been well studied, few studies have optimized SPE for effect-based methods. The aim of the current study was to develop and evaluate two standard operating procedures (SOPs) for the enrichment of micropollutants in preparation for chemical analysis and bioanalysis, one covering a broad range of chemicals and the other selective for estrogenic chemicals. Results: Pristine surface water spiked with > 600 micropollutants was used to develop a generic extraction method for micropollutants with a wide range of physiochemical properties, while water spiked with estrogenic chemicals was used to identify a selective extraction method. Three different SPE sorbents were tested, with recoveries of individual chemicals and effect in assays indicative of mutagenicity, estrogenic activity, and fish embryo toxicity assessed. The sorbent HRX at pH 7 was selected for the generic extraction method as it showed the best recovery of both individual chemicals and effect in the bioassays. The sorbent HLB at pH 3 showed optimal recovery of estrogenic chemicals and estrogenic activity. The two optimal SPE methods were applied to spiked and unspiked wastewater effluents, with the concentrations of detected chemicals and observed effects similar to those of previous studies. The long-term storage of both extracts and SPE cartridges for estrogens and estrogenic activity after extraction with the HRX and HLB methods were evaluated, with estrogenic effectiveness close to 100% after 112 days when HLB was used. Conclusions: HRX is recommended for generic extraction, while HLB is optimal for the selective extraction of estrogenic micropollutants. However, if a laboratory only wants to use a single SPE sorbent, HLB can be used for both generic and selective extraction as it yielded similar chemical and effect recovery as HRX for a wide range of micropollutants. This paper is supplemented by the final SOP that includes a variant for generic extraction and one for the extraction of estrogenic chemicals. [ABSTRACT FROM AUTHOR]

Acrylamide is a hazardous chemical mainly synthesized during the thermal processing of foods representing a significant concern within the broader issue of food contaminants and their impact on public health. Acrylamide can be absorbed by the human body through dietary intake, respiration, dermal contact, and mucosa. The metabolic conversion of acrylamide into mercapturic acid metabolites and glycidamide results in several adverse and toxic effects. Therefore, this review explores the formation, toxicity, and metabolism of acrylamide. Hence, it is crucial to detect and ensure product quality via risk evaluation. Traditional analytical techniques for acrylamide detection often require expensive instrumentation and complex sample preparation, prompting the exploration of alternative, cost‐effective, sustainable methods. Here, we propose the utilization of carbon quantum dots (CQDs) synthesized through green approaches as a novel solution. CQDs display their immense potential for diverse applications due to their valuable properties such as biocompatibility, photocatalysis, and strong fluorescence. This review highlights the distinct potential of CQDs as a fluorescence probe for detecting acrylamide, showcasing their efficacy in addressing food safety concerns. In addition, various extraction and purification techniques for acrylamide such as QuEChERS, solid phase extraction, Carrez clarification, and dispersive liquid‐liquid microextraction are comprehensively reviewed. QuEChERS is regarded as a most promising technique for the extraction of acrylamide owing to its cost‐effective, rapid, and higher recovery rates. [ABSTRACT FROM AUTHOR]

Because residues of chlorpyrifos being the most common in vegetables that are generally consumed uncooked and the demand for healthy vegetables has increased, an effective approach to remove these residues from vegetables is necessary. This study aimed to determine how effectively chlorpyrifos residues could be removed from a variety of vegetables by utilizing low concentrations of ozonated water as a green technology over different contact times. Solid-phase extraction was employed, and then residues were analyzed using GC‒MS. The study illustrated that the initial concentration of chlorpyrifos residues in arugula > parsley > leek > tomato > carrot > cucumber > cabbage > bell pepper. The % chlorpyrifos removal ranged 30–83, 91–97, 80–92, 92–95, 87–97, 95–97, 64–100, and 90–97% for bell pepper, tomato, cucumber, carrot, arugula, parsley, cabbage, and leek, respectively. A first-order kinetic model was assumed to explore the removal of chlorpyrifos and degradation rate constants increased as follows: parsley > carrot ≈ leek > arugula > tomato > cucumber > cabbage > bell pepper, with the absence of the chlorpyrifos-oxon which is more toxic than the parent chlorpyrifos after ozone treatments. Importantly, the use of ozonated water for chlorpyrifos removal had no appreciable adverse effects on the total phenolic compound, vitamin C levels, or free radical scavenging activity in most of the tested vegetables. These findings imply that ozone technology is a safe and effective method for eliminating chlorpyrifos from the surface of vegetables, potentially lowering the risk to consumer health. [ABSTRACT FROM AUTHOR]

Therapeutic drug monitoring is essential for ensuring the efficacy and safety of medications. This study introduces a streamlined approach that combines pipette-tip solid-phase extraction (PT-SPE) with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), facilitating rapid and high-throughput monitoring of drug concentrations. As a demonstration, this method was applied to the extraction and quantification of antidepressants in serum. Utilizing Zip-Tip C18, the method enabled the extraction of antidepressants from complex biological matrices in less than 2 min, with the subsequent MALDI-MS analysis yielding results in just 1 min. Optimal extraction recoveries were achieved using a sampling solution at pH 9.0 and a 10 μL ethanol desorption solution containing 0.1% phosphoric acid. For MALDI analysis, 2,5-dihydroxybenzoic acid was identified as the most effective matrix for producing the highest signal intensity. The quantification strategy exhibited robust linearities (R2 ≥ 0.997) and satisfactory limits of quantification, ranging from 0.05 to 0.5 μg/mL for a suite of antidepressants. The application for monitoring dynamic concentration changes of antidepressants in rat serum emphasized the method's efficacy. This strategy offers the advantages of high throughput, minimal sample usage, environmental sustainability, and simplicity, providing ideas and a reference basis for the subsequent development of methods for therapeutic drug monitoring. [ABSTRACT FROM AUTHOR]

Copyright of Food & Fermentation Industries is the property of Food & Fermentation Industries and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

AbstractAn efficient and innovative clean-up method was developed for the rapid screening of β-agonists residues in porcine urine by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). 1% Aqueous ammonium hydroxide was shown to be effective for the removal of matrix components as a wash step in solid phase extraction (SPE). A significant reduction in matrix effects was observed with values from 81% to 108%. Furthermore, under the optimized conditions, the recoveries of all analytes at 0.3, 0.6, and 3.0 μg/L ranged from 70.1% to 109.0% when employing the external standard method for quantitative analysis, rather than relying on matrix-matched standards or isotope-labelled internal standards to mitigate matrix effects. The limits of detection (LOD) and limits of quantification (LOQ) were 0.1 μg/L and 0.3 μg/L, respectively. This method has been successfully applied to screen β-agonists in porcine urine and is a promising tool for multi-residue analysis. [ABSTRACT FROM AUTHOR]

The presence of PFAS in drinking water may pose a serious threat to human health. This study aims to determine the levels of these compounds and their precursors in water samples from a drinking water treatment plant (DWTP) located in l'Ampolla (Spain) and to assess their fate. Additionally, ten Spanish bottled waters were analyzed to compare the occurrence of PFAS in the mentioned matrices and in drinking water. Off-line solid phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) was applied to determine 26 PFAS and PFAS precursors after a total oxidizable precursor assay. The analytical method presents low quantification limits (0.25–5 ng/L). A total PFAS concentration of up to 16 ng/L in all the DWTP samples was obtained, and 6:2 FTS was the only precursor detected. Results are close to the quantification limits, resulting in a high degree of uncertainty, and for this, it is difficult to evaluate the DWTP PFAS removal efficiency. Regarding bottled water, total PFAS concentration found was up to 12 ng/L in one of ten samples, with no precursors detected. Exposure assessment revealed that there is no risk associated with the ingestion of the samples analyzed. Moreover, there were no differences in terms of risk between drinking water from l'Ampolla DWTP and bottled water. [ABSTRACT FROM AUTHOR]

The detection and quantification of hormones are important to assess the reproductive and stress status of experimental models and for the diagnosis of diseases in human and veterinary clinics. Traditionally, steroid, peptide, and protein hormones are analyzed in individual experiments using different extraction methodologies. With the new advancement on HPLC sorbents, the simultaneous measurement of hormones from different categories becomes possible. In this study, we present a novel sample processing strategy for the simultaneous extraction and detection of peptides, steroids, and proteins using high-resolution liquid chromatography tandem mass spectrometry. We demonstrate the sensitivity of our method for small tissues by acquiring data from brain, pituitary gland, and gonads of single zebrafish samples. This approach promises to shed light on the hormonal pathways and their interrelationships, providing knowledge on the integration of hormone systems. [ABSTRACT FROM AUTHOR]

The global spread of multidrug-resistant Escherichia coli threatens human, animal, and environmental health. Despite the recognition of water bodies as potential reservoirs, research on antimicrobial resistance (AMR) and antibiotic residues in the Baltic Sea is limited. In this study, we examined the presence of ESBL-producing E. coli in surface water in northeastern Germany. We then conducted phenotypic and genotypic analyses of the strains, which encompassed AMR and heavy metal/metalloid tolerance, biofilm formation, and detailed plasmid examination. In addition, we used solid-phase extraction with ultra-high performance liquid chromatography and mass spectrometry to quantify antibiotic residues. Our analysis identified 30 ESBL-producing E. coli isolates, some of which were associated with clinically relevant high-risk clonal lineages. We detected antibiotic residues in the environmental samples, but the antibiotic concentrations were significantly lower compared to wastewater samples. These results suggest that the Baltic Sea surface water could serve as a reservoir for ESBL-producing E. coli and clinically relevant antibiotics. [ABSTRACT FROM AUTHOR]

Despite advancements in the sensitivity and performance of analytical instruments, sample preparation remains a bottleneck in the analytical process. Currently, solid-phase extraction is more widely used than traditional organic solvent extraction due to its ease of use and lower solvent requirements. Moreover, various microextraction techniques such as micro solid-phase extraction, dispersive micro solid-phase extraction, solid-phase microextraction, stir bar sorptive extraction, liquid-phase microextraction, and magnetic bead extraction have been developed to minimize sample size, reduce solvent usage, and enable automation. Among these, in-tube solid-phase microextraction (IT-SPME) using capillaries as extraction devices has gained attention as an advanced "green extraction technique" that combines miniaturization, on-line automation, and reduced solvent consumption. Capillary tubes in IT-SPME are categorized into configurations: inner-wall-coated, particle-packed, fiber-packed, and rod monolith, operating either in a draw/eject system or a flow-through system. Additionally, the developments of novel adsorbents such as monoliths, ionic liquids, restricted-access materials, molecularly imprinted polymers (MIPs), graphene, carbon nanotubes, inorganic nanoparticles, and organometallic frameworks have improved extraction efficiency and selectivity. MIPs, in particular, are stable, custom-made polymers with molecular recognition capabilities formed during synthesis, making them exceptional "smart adsorbents" for selective sample preparation. The MIP fabrication process involves three main stages: pre-arrangement for recognition capability, polymerization, and template removal. After forming the template-monomer complex, polymerization creates a polymer network where the template molecules are anchored, and the final step involves removing the template to produce an MIP with cavities complementary to the template molecules. This review is the first paper to focus on advanced MIP-based IT-SPME, which integrates the selectivity of MIPs into efficient IT-SPME, and summarizes its recent developments and applications. [ABSTRACT FROM AUTHOR]

Abnormal levels of catecholamine (CA) neurotransmitters and their metabolites in biological fluids can lead to various neurological disorders. Herein, a boric acid‐functionalized hypercrosslinked polymer was prepared and utilized as a sorbent for the dispersive solid‐phase extraction of CAs and their metabolites in rat serum. By combination with a high‐performance liquid chromatography‐fluorescence detector, the extraction parameters for the seven target analytes were optimized. Under the optimal extraction condition, the methodology for the quantitative analysis of CAs and their metabolites in rat serum samples was established. The limits of detection and limits of quantification were found to be in the ranges of 0.010–0.015 and 0.033–0.050 ng/mL, respectively. The results demonstrated satisfactory recoveries, with values ranging from 88.02% to 113.27%, accompanied by relative standard deviations within the range of 2.69%–9.59%. In addition, the method showed good anti‐interference ability (matrix effect ranged from 2.64% to 18.07%). The developed method was validated for the determination of CAs and their metabolites in normal and Alzheimer's disease model rats' serum, which proved the promising application of the method for CAs neurotransmitter analysis in biological samples. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Shipin Kexue/ Food Science is the property of Food Science Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

A growing environmental concern revolves around the widespread use of medicines, particularly antibiotics, which adversely impact water quality and various life forms. The unregulated production and utilization of antibiotics not only affect non-targeted organisms but also exert significant evolutionary pressures, leading to the rapid development of antimicrobial resistance (AMR) in bacterial communities. To address this issue, global studies have been conducted to assess the prevalence and quantities of antibiotics in various environmental components including freshwater, ocean, local sewage, and fish. These studies aim to establish effective analytical methods for identifying and measuring antibiotic residues in environmental matrices that might enable authorities to establish norms for the containment and disposal of antibiotics. This article offers a comprehensive overview of methods used to extract antibiotics from environmental matrices exploring purification techniques such as liquid–liquid extraction, solid-phase extraction, green extraction techniques, and concentration methods like lyophilization and rotary evaporation. It further highlights qualitative and quantitative analysis methods, high-performance liquid chromatography, ultra-high-performance liquid chromatography, and liquid chromatography-tandem along with analytical methods such as UV–Vis and tandem mass spectrometry for detecting and measuring antibiotics. Urgency is underscored for proactive strategies to curb antibiotic contamination, safeguarding the integrity of aquatic ecosystems and public health on a global scale. [ABSTRACT FROM AUTHOR]

Graphite carbon nitride (g-C3N4) is a two-dimensional nano-sheet with electronic properties, which shows unique characteristics with high chemical and thermal stability in its structure. The functionalization of these compounds through covalent bonding is an important step towards significantly improving their properties and capabilities. To achieve this goal, a novel strategy for the covalent functionalization of Fe3O4@g-C3N4 with thiamine hydrochloride (vitamin B1) via cyanuric chloride (TCT), which is a divalent covalent linker, was presented. The efficiency of Fe3O4@gC3N4@Thiamine as a heterogeneous organic catalyst in the synthesis of spirooxindole-pyran derivatives and 2-amino-4H-pyran under solvent-free conditions was evaluated and the yields of high-purity products were presented. In addition, easy recycling and reuse for seven consecutive cycles without significant reduction in catalytic activity are other features of this catalyst. Moreover, the performance of the prepared sorbent in the microextraction technique (herein, magnetic solid phase extraction) was studied. The tebuconazole was selected as the target analyte. The target analyte was extracted and determined by HPLC–UV. Under the optimum condition, the linear range of the method (LDR) was estimated in the range of 0.2–100 μg L−1 (the coefficient of determination of 0.9962 for tebuconazole). The detection limit (LOD) of the method for tebuconazole was calculated to be 0.05 µg L−1. The limit of quantification (LOQ) of the method was also estimated to be 0.16 µg L−1. In order to check the precision of the proposed method, the intra-day and inter-day relative standard deviations (RSD%) were calculated, which were in the range of 1.5- 2.8%. The method was used for the successful extraction and determination of tebuconazole in tomato, cucumber, and carrot samples. [ABSTRACT FROM AUTHOR]

AbstractCanthaxanthin and β-apo-8’-carotenoid ethyl ester are widely used as feed additives in poultry feed for enhancing the color of poultry products. The excessive intake of the two colorants can cause health damage. According to the European Food Safety Authority (EFSA), the acceptable daily intake (ADI) of canthaxanthin and β-apo-8’-carotenoid ethyl ester are 0.03 mg/kg·bw and 0.015 mg/kg·bw, respectively. Ultra-high-performance liquid chromatography-diode array detector (UPLC-DAD) was used to determine two colorants in chicken eggs and meat. A PRiME HLB solid-phase extraction cartridge was used to extract and clean-up the sample. BEH C18 column was used as the separation column, with water containing 0.1% formic acid and acetonitrile as the mobile phase. The limit of detection (LOD) was 0.05 mg/kg, and the limit of quantification (LOQ) was 0.1 mg/kg. The recoveries were between 90% and 104%. The daily intake of two colorants in chicken eggs and meat was evaluated based on the detection data, food consumption data and weight data of the population. The mean estimated daily intake (EDI) values of canthaxanthin through chicken eggs and meat were 1.09 µg/(kg·bw·d) and 0.013 µg/(kg·bw·d), respectively. The mean EDI value of β-apo-8’-carotenoid ethyl ester through eggs was 0.44 µg/(kg·bw·d). The results showed that eggs were the main contributor to the daily intake of two colorants. The mean hazard quotients (HQ) values of two colorants through chicken eggs and meat was within a safe range. [ABSTRACT FROM AUTHOR]

This work introduces a novel method of recovering bioactive berry natural products (BNPs) using solid phase extraction with metal‐organic frameworks (MOF‐SPE). Two pyrene‐based MOFs with different structural topologies, Al‐PyrMOF and Zr‐NU‐1000, were evaluated for their ability to capture and desorb BNPs, including ellagic acid, quercetin, gallic acid, and p‐coumaric acid. Time‐dependent BNP uptake via dispersive SPE revealed that NU‐1000 outperformed Al‐PyrMOF in capturing all BNPs. Our findings show NU‐1000 demonstrated a higher and more consistent BNP capture profile, achieving over 90 % capture of all BNPs within 36 h, with only a 9 % variation between the most and least effectively captured BNPs. In contrast, Al‐PyrMOF, displayed a staggered uptake profile, with a significant 53 % difference in capture efficiency between the most and least effectively captured BNP. However, when a BNP mixture was used at a loading concentration of 50 μg/mL, Al‐PyrMOF outperformed NU‐1000, capturing over 70 % of all BNPs. Al‐PyrMOF also exhibited improved BNP recovery, with a minimum of two‐fold greater amount recovered for all BNPs. Further testing with a BNP mixture at a concentration of 15 μg/mL demonstrated that Al‐PyrMOF efficiently concentrated all BNPs, achieving a maximum extraction factor of 2.71 observed for quercetin. These findings highlight the use of Al‐PyrMOF as a MOF‐SPE sorbent for recovering bioactive BNPs. [ABSTRACT FROM AUTHOR]

AbstractMethiocarb is a carbamate pesticide and is widely used due to its short lifetime but is a health concern due to its toxicity. To address this challenge, a novel nano-sorbent (zinc aluminate hybrid doped onto a magnetic activated carbon cloth (magnetic ACC@ZnAl2O4)) was synthesized. The characterization of the composite was done using FTIR spectroscopy, SEM, XRD, and EDX. The synthesized composite was then employed for the efficient extraction of methiocarb from food samples. Under the optimum conditions of (pH: 7.0, vortex time: 0.5 min, adsorbent dose: 5 mg, initial volume of sample: 50 mL, volume of eluent: 1.0 mL), quantitative recovery values of methiocarb in food samples were obtained (80–114%). This method impresses with its exceptional sensitivity, achieving incredibly low detection (LOD: 20 µg L−1) and quantification (LOQ: 67 µg L−1) limits for methiocarb. Its efficiency is equally impressive, with high values of preconcentration factor (PF: 50) and enhancement factor (EF: 49.4), ensuring accurate and reliable analysis with a low value of relative standard deviation (RSD: 4.8%). The method’s impressive selectivity, evident in its minimal interference from other pesticides, paves the way for reliable methiocarb analysis in food samples. [ABSTRACT FROM AUTHOR]

This scoping review intends to identify the most used analytical methods and biological samples in the post-mortem forensic toxicological analysis of cocaine and its metabolites. A scoping review was performed based on the question "What are the analytical methods and types of biological samples most frequently used to identify and quantify cocaine in post-mortem forensic toxicology?" The studies were selected from five databases and, after exclusions, the data were tabulated, analyzed, and reported. Twenty-one articles published between 2012 and 2022 were filtered from five different databases to be studied. The collected data indicate that the most used biological samples were blood and hair. The most used sample preparation technique was solid phase extraction, while the most mentioned chromatography method was liquid chromatography with mass spectrometry. This review presents and discusses the state of the art regarding methods for the detection sensitivity spectrum, why limits of quantification are so important for these methods, and what are the most suitable biological samples to be utilized in each case. Cocaine and metabolites are important in forensic toxicologic post-mortem analysis. However, there is little concern in the development of miniaturized and automated sample preparation in this field. Besides, there is not enough understanding of post-mortem redistribution, tolerance, drug-drug interactions, and pre-existing medical conditions. [ABSTRACT FROM AUTHOR]

A method to determine aceclofenac, ketorolac, and sulindac in human urine samples using microemulsion electrokinetic chromatography (MEEKC) has been developed in this study. The optimization of MEEKC conditions was carried out by changing the microemulsion compositions including the buffer pH, borate salt concentration, surfactant concentration, co-surfactant concentration, organic modifier concentration, and oil droplet concentration. The optimum separation of selected drugs was obtained with a composition of microemulsion containing 10 mM borate buffer pH 9, 0.5% sodium dodecyl sulphate (SDS), 6.6% n-butanol, 6.0% acetonitrile, and 0.8% ethyl acetate. Excellent linearity was obtained in the range concentration of 25 to 200 ppm with r2 > 0.999. Limits of detection (LOD, S/N = 3) and limits of quantification (LOQ, S/N = 10) were 2.72 to 4.75 and 9.08 to 15.85 ppm, respectively. The solid-phase extraction (SPE) method using C-18 as an adsorbent and the solid phase micro-tip extraction (SPMTE) method using multiwalled carbon nanotubes (MWCNTs) as an adsorbent were used to clean-up and pre-concentrate the urine samples prior to the MEEKC analysis. The best recoveries of the selected drugs in the spiked urine sample were 91 to 103% with RSD of 1.26 to 4.03% (n = 3) using the SPE-MEEKC method. [ABSTRACT FROM AUTHOR]

Τhyreostats (TSs) are veterinary drugs used in livestock farming for fattening. Their administration is banned in the European Union since 1981, and their monitoring for food quality and safety control requires sensitive and confirmatory methods. The present study describes the development and validation of a hydrophilic interaction liquid chromatography tandem mass spectrometry (HILIC-MS/MS) method for the simultaneous determination of 2-thiouracil (TU), 6-methyl-2-thiouracil (MTU), 6-propyl-2-thiouracil (PTU), 6-phenyl-2-thiouracil (PhTU), tapazole (TAP), and 2-mercaptobenzimidazole (MBI) in bovine muscle tissues. Investigation of the retention mechanism of the six analytes on the selected amide-based stationary phase showed that hydrophilic partition was the dominant interaction. The sample preparation included extraction with ACN/H2O (80/20), followed by dispersive solid-phase extraction (d-SPE) with C18 sorbent and hexane partitioning. The method was validated according to European guidelines using internal standards, including isotopically labelled ones. The method's LODs ranged between 2.8 ng g−1 (6-phenyl-2-thiouracil) and 4.1 ng g−1 (2-thiouracil). Application of the proposed method to 48 bovine tissue samples showed non-detectable results. [ABSTRACT FROM AUTHOR]

Short-chain fatty acids (SCFAs) in feces are inextricably linked to intestinal homeostasis and can be used as potential markers for metabolic diseases. In this study, an efficient and simple method was developed for the purification of SCFAs without the need for derivatization of the samples. The SCFAs (acetic, propionic, isobutyric, butyric, isovaleric, valeric, and hexanoic acid) were extracted from a small amount (50 mg) of fecal and intestinal samples using acetone combined with solid phase extraction column (Bond Elut Plexa) enrichment. Quantitative analysis was performed using gas chromatography with a flame ionization detector. The developed method has shown very good limits of detection (LOD, 0.11–0.36 μM) and limits of quantification (LOQ, 0.38–1.21 μM) with excellent linearity (R2 ≥ 0.9998), good recovery (98.34–137.83%), and high reproducibility (RSD ≤ 1.30). The applicability of this method was also demonstrated by testing the fecal and cecum contents of different species from mammals (mice, pigs) to insects (honeybees). The technique is highly suitable for analyzing complex, small amounts of intestinal and fecal SCFAs. [ABSTRACT FROM AUTHOR]

A simple, fast, and low-cost pre-concentration methodology based on the application of solid-phase extraction coupled to layered double hydroxides (LDHs) and capillary electrophoresis was developed for the determination of naproxen (NPX), diclofenac (DFC), and ibuprofen (IBP) in environmental sample waters. A systematic study of the LDH composition was designed, including the effects of interlayer anions (NO3−, Cl−, CO32−, BenO−, and SDS−) and the effect of molar ratio (Mg:Al). The optimal composition of MgAl/Cl−-LDH (Mg:Al; 1.5:1.0) was coupled to an SPE system: pH (neutral pH), LDH amount (15 mg), and extraction capacity ranged from 79.71 to 83.11% for the three anti-inflammatory non-steroidal agents analyzed. A recovery rate of up to 80.87% was obtained when 0.01 M chloride acid in methanol was used as the eluent and 50 mL of sample was used. Under optimal conditions, the linear range of the calibration curve ranges from 18.02 to 200 μg L−1, with limits of detection ranging from 6.03 to 18.02 μg L−1 for the three NSAIDs. The precision of the methodology was evaluated in terms of inter- and intra-day repeatability, with %RSD < 10% in all cases. The proposed method was applied to analyze environmental water samples (bottle, tap, cistern, well, and river water samples). The developed method is a robust technique capable of combining with other analytical methods to quantitatively determine anti-inflammatory non-steroidal agents. [ABSTRACT FROM AUTHOR]

Phospholipids (PLs), essential components of cell membranes, play significant roles in maintaining the structural integrity and functionality of joint tissues. One of the main components of synovial joint fluid (SJF) is PLs. Structures such as PLs that are found in low amounts in biological fluids may need to be selectively enriched to be analyzed. Monodisperse-mesoporous SiO2 microspheres were synthesized by a multi-step hydrolysis condensation method for the selective enrichment and separation of PLs in the SJF. The microspheres were characterized by SEM, XPS, XRD, and BET analyses. SiO2 microspheres had a 161.5 m2/g surface area, 1.1 cm3/g pore volume, and 6.7 nm pore diameter, which were efficient in the enrichment of PLs in the SJF. The extracted PLs with sorbents were analyzed using Q-TOF LC/MS in a gradient elution mode with a C18 column [2.1 × 100 mm, 2.5 μM, Xbridge Waters (Milford, MA, USA)]. An untargeted lipidomic approach was performed, and the phospholipid enrichment was successfully carried out using the proposed solid-phase extraction (SPE) protocol. Recovery of the SPE extraction of PLs using sorbents was compared to the classical liquid–liquid extraction (LLE) procedure for lipid extraction. The results showed that monodisperse-mesoporous SiO2 microspheres were eligible for selective enrichment of PLs in SJF samples. These microspheres can be used to identify PLs changes in articular joint cartilage (AJC) in physiological and pathological conditions including osteoarthritis (OA) research. [ABSTRACT FROM AUTHOR]

The global rise of new psychoactive substances (NPSs) poses challenges for their analysis in biological matrices due to their complex chemistries and short market lifespan. A comparative study for the simultaneous extraction, separation, and detection of 19 NPSs was conducted. Six solid-phase extraction (SPE) methods and one supported liquid extraction method (SLE) were compared for the extraction of analytes from blood, serum, plasma, and urine. Comparisons of four derivatization agents were conducted, at four temperatures and two incubation times. Extraction methods were assessed by precision, sensitivity, and extraction efficiency. Derivatizing agents were assessed on their selectivity and sensitivity, and a three-way ANOVA was conducted to determine statistical significance. CSDAU SPE cartridges were shown to be the most efficient when extracting analytes from blood, serum, and plasma, whereas Xcel I cartridges performed the strongest when extracting analytes from urine. SPE extraction efficiencies, when utilizing the best-performing cartridges, ranged from 49 to 119%. SLE successfully extracted all analytes from all matrices (ranging from 22 to 120%). Pentafluoropropionic anhydride: ethyl acetate was the most successful derivatizing agent, allowing all analytes to be detected, with the highest peak area responses and more unique spectra. The optimum temperature for incubation was 37 °C, with no statistical difference found between the two incubation times. [ABSTRACT FROM AUTHOR]

Pharmaceuticals in the environment are a global concern, with studies in all continents highlighting their widespread occurrence and potential ecological impacts, revealing their presence, fate, and associated risks in aquatic ecosystems. Despite typically occurring at low concentrations (ranging from ng/L to µg/L), advancements in analytical methods and more sensitive equipment have enabled the detection of a higher number of pharmaceuticals. In this study, surface and wastewater samples were extracted using solid phase extraction and analyzed using ultra-high-performance liquid chromatography with tandem mass spectrometry. Among the therapeutic classes investigated, nonsteroidal anti-inflammatory drugs/analgesics, antibiotics, and psychiatric drugs showed a higher number of detected pharmaceuticals. Concentrations ranged from below method detection limit (

Background As one of the speculated bisphenols to replace bisphenol A (BPA), bisphenol F (BPF), naturally present in mustard, is structurally similar to BPA and may have similar estrogenic activity, but information on its toxicity is very limited compared to BPA. Objective In order to support the toxicology study of BPF at Heath Canada, a GC–MS method based on solid-phase extraction (SPE) and derivatization was developed for analysis of BPF in liver samples. Methods Samples were treated with β-glucuronidase to convert BPF glucuronide to free BPF for analysis of total BPF. Results The method was validated for free BPF at different spiking levels, and recoveries ranged from 90–97.5% with RSDs from 0.11–5.54%. The method was also validated for glucuronide-conjugated BPF at different spiking levels of BPF mono-β-D-glucuronide: recoveries ranged from 72.3–93.3% with RSDs from 1.7–8.94%. The method was used to analyze 60 liver tissue samples from rats dosed with BPF at different levels in a toxicology study. Free and glucuronide-conjugated BPF were not detected in any of the control samples, which were not dosed with BPF (average method detection limit: 0.31 ng/g) but detected in all the other liver tissue samples with levels increasing at higher doses. The percentage of glucuronide-conjugated BPF in total BPF varied among the liver samples, from as low as 9.8% to as high as 77.9%, indicating the importance of analyzing biological samples for BPF in both free and conjugated forms for total exposure. Conclusion A GC–MS method based on solid-phase extraction (SPE) and derivatization was developed for analysis of both free and glucuronide-conjugated BPF in liver samples. This method was validated not only for free BPF, but also for mono-β-D-glucuronide-conjugated BPF for the first time to confirm the efficiency of the deconjugation procedure with enzyme. Highlights This method can be adapted and applied for analysis of free and glucuronide-conjugated BPF in other biological samples with appropriate validation in target sample matrixes. [ABSTRACT FROM AUTHOR]

This study investigated the composition of the aroma substances and the physicochemical properties of lyophilized coffee produced from Ecuador Arabica and robusta coffee beans. In the present study, we propose a fast method of analyzing volatile compounds in coffee using the headspace solid phase extraction method (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). According to the results, 25 aroma compounds were detected in coffee, the most important of which are 2-acetylfuran, 2-furanmethanol, 2,3-dimethylpyrazine, 2,3,5-trimethylpyrazine, and 2-methoxy-4-vinylphenol. As is known, furans and pyrazines are associated with "roasted, cocoa, coffee, and hazelnut" odours. The most important organic acids detected in the study are citric, maleic, and succinic. [ABSTRACT FROM AUTHOR]

A magnetic solid-phase extraction method with the dispersion of magnetic hypercrosslinked polystyrene (MHCPS) by carbon dioxide is proposed for the extraction and preconcentration of amphenicols (chloramphenicol, florfenicol, and thiamphenicol) from honey and milk before their determination by HPLC–MS/MS. Effervescent tablets, consisting of sodium bicarbonate, citric acid, and MHCPS in the case of honey and sodium bicarbonate and MHCPS in the case of milk, were used. The conditions for obtaining tablets were selected (the amount and ratio of the acid, base, and MHCPS in the composition of a tablet and its mass), ensuring the quantitative release of amphenicols. Procedures for the determination of amphenicols in honey and milk with the dispersion of the sorbent by carbon dioxide and the subsequent determination of the compounds by HPLC–MS/MS are developed. The limits of detection are 0.3–1 and 0.02–0.05 μg/kg for honey and milk, respectively. [ABSTRACT FROM AUTHOR]

Sample preparation is one of the viable procedures to be used before analysis to enhance sensitivity and reduce the matrix effect. The current review is mainly emphasized the latest outcome and applications of microextraction techniques based on the miniaturization of the classical conventional methods based on liquid-phase and solid-phase extraction for the quantitative elemental analysis in different real samples. The limitation of the conventional sample preparation methods (liquid and solid phase extraction) has been overcome by developing a new way of reducing size as compared with the conventional system through the miniaturization approach. Miniaturization of the sample preparation techniques has received extensive attention due to its extraction at microlevels, speedy, economical, eco-friendly, and high extraction capability. The growing demand for speedy, economically feasible, and environmentally sound analytical approaches is the main intention to upgrade the conventional procedures apply for sample preparation in environmental investigation. A growing trend of research has been perceived to quantify the trace for elemental analysis in different natures of real samples. This review also recapitulates the current futuristic scenarios for the green and economically viable procedure with special overemphasis and concentrates on eco-friendly miniaturized sample-preparation techniques such as liquid-phase microextraction (LPME) and solid-phase microextraction (SPME). This review also emphasizes the latest progress and applications of the LPME and SPME approach and their future perspective. [ABSTRACT FROM AUTHOR]

Sulfonylurea herbicides (SUHs) are widely used in agriculture because of their low dosage, low cost, and high selectivity. However, due to improper use and lack of effective management, their residues pose a threat to the human health through environment and food pollution. Therefore, there is a need for simple, quick, economical, and effective methods to analyze SUHs in plant-derived foods, crops, and environmental samples. The present article presents a comprehensive review of the pretreatment and analytical technologies used for SUHs in various sample matrices, focusing on the developments since 2010. The main pretreatment methods include liquid–liquid extraction, solid-phase extraction, QuEChERS, and different microextraction methods, whereas analytical methods mainly include liquid chromatography coupled with different detectors, capillary electrophoresis, among others. In addition, the present study also compared the advantages and disadvantages of the methods and the future development is prospected. Highlight: Progress in pretreatment and analytical methods of sulfonylurea herbicides are summarized. Pros and cons of the pretreatment and determination methods have been given. Novel materials in solid-phase extraction and solid-phase microextraction are depicted. [ABSTRACT FROM AUTHOR]

Xylazine has emerged in recent years as a dangerous adulterant in illicit fentanyl use, and methods for the detection of xylazine in toxicology panels are still lagging. We developed methods for the screening and quantitation of xylazine in oral fluid (OF), a popular testing medium due to its ease of collection and reflection of presence in blood for many classes of drugs. Enzyme-linked immunosorbent assays were employed for the rapid screening of xylazine directly from the collection device buffer with a cutoff of 1 ng/mL. Solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry facilitated the confirmation and quantification of xylazine as low as 0.1 ng/mL and a dynamic range of 0.1–25 ng/mL. Selectivity, ionization suppression, processed sample stability, and dilution effect were also assessed. The method was validated through the American National Standards Institute/American Academy of Forensic Sciences Standards Board (ANSI/ASB) Standard 036, first edition from 2019, and found to be accurate, precise, and robust. Living human subject OF samples collected within substance use disorder and therapeutic drug monitoring clinics received between September 2023 and January 2024, with the specific request to test for xylazine (n  = 57), were screened. Presumptive positive samples were confirmed using the validated method. Xylazine confirmed living human subject OF sample concentrations ranged from 1.2 to 23.3 ng/mL. [ABSTRACT FROM AUTHOR]

This review article describes some of the recent advances in ultra‐trace determination of uranium in various natural water bodies such as drinking water, underground water, seawater, etc. using total reflection x‐ray florescence (TXRF) spectrometry. Uranium is one of the most hazardous element having chemical as well as radio‐toxicity. However, due to its low concentration in water samples, direct determination is seldom possible in samples with high salt content. Various sample preconcentration and selective extraction techniques for uranium such as solvent extraction, dispersive liquid–liquid micro extraction, solid phase extraction, and membrane based preconcentration methods are summarized in this article. TXRF is a very versatile micro‐analytical technique with detection limits in picogram range and having multielemental analysis capability. TXRF determination of uranium using U Lα as the analytical line has many analytical challenges and difficulties, mainly due to the severe interference with Rb and Br, both are commonly available in natural water samples. This article highlights some of these challenges, along with the advantages and disadvantages of the different sample preparation techniques used so far for uranium determination in natural water samples by TXRF. [ABSTRACT FROM AUTHOR]

The applicability of two layered double hydroxide adsorbents, that is, Zn/Al LDH and the reduced graphene oxide-modified Zn/Al-rGO LDH for the solid phase extraction-preconcentration of naproxen followed by HPLC determination is evaluated and compared. The adsorbents are characterized by using XRD, FT-IR, FE-SEM, BET, and TEM techniques. The optimization of parameters affecting the extraction procedure included pH and sample solution volume, amount of the adsorbents, adsorbent/sample solution contact time, type, concentration, and volume of the desorption solution, and the time required for desorption process was performed by using univariate method. It is assumed that the uptake of anionic form of naproxen is taken place via the ion exchange mechanism with interlayer carbonate anions of the studied LDHs. The applicability of the adsorbents is evaluated by the determination of naproxen in human urine, hospital, and pharmaceutical wastewater samples. The obtained linear ranges by employing the unmodified and modified LDHs for the determination of naproxen in pharmaceutical wastewater were found to be 10–530 µg L−1 (R2 = 0.9999) and 5–630 µg L−1 (R2 = 0.9999), respectively. The limits of detection and enrichment factor were appraised as 5.1 µg L−1 and 42 by employing Zn/Al LDH, and 3.1 µg L−1 and 54.5 by using Zn/Al-rGO LDH. Both investigated LDHs are able to be used in solid phase extraction-preconcentration of naproxen in real samples. However, the evaluated figures of merit reveal that the modified Zn/Al-rGO LDH is more efficient adsorbent than the unmodified Zn/Al LDH for the extraction of naproxen. [ABSTRACT FROM AUTHOR]

Matrix effects are a major concern in liquid chromatography coupled to tandem mass spectrometry for the determination of pesticide residues. In this work, a novel and efficient lipophilicity-matched chromatographic separation strategy was developed to improve the separation efficiency on an alkyl bonded phase chromatographic column and reduce matrix effects. An ultra-high performance liquid chromatography-tandem mass spectrometry method based on this strategy was established to minimize matrix effects for the determination of triazole fungicides. The samples were cleaned-up with dispersive solid phase extraction and separated on a chromatographic column with similar lipophilicity to the fungicides. The results showed that the proposed method effectively minimized the matrix effects and improved the separation. The matrix effects of 21 fungicides ranged from −8.3% to 4.7%. Moreover, the average recoveries were between 91.4% and 108.1% using solvent calibration for quantification, and the limits of quantitation were between 0.5 and 3.5 μg/kg. These results demonstrate the effectiveness of the proposed strategy in improving the chromatographic efficiency. This work provides a practical strategy and reference for the liquid chromatography-tandem mass spectrometry determination of pesticide residues. [ABSTRACT FROM AUTHOR]

A rapid and effective method utilizing ultrasonic assisted-dispersive solid-phase microextraction coupled with gas chromatography/mass spectrometry (GC/MS) was developed for the determination of lorazepam and diazepam in biological and aqueous samples. A modified nanocrystalline cellulose-based sorbent was prepared and applied for the microextraction of the analytes. The extraction efficiency of the sorbents prepared using self-assembled N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, including cellulose nanostructure and modified nanocrystalline cellulose, was compared. The modified cellulose nanostructure was characterized using thermogravimetric analysis (TGA), energy dispersive X-ray (EDX), and Fourier transform infrared spectroscopy (FTIR). Additionally, the study investigated the effects of relevant factors on the extraction/desorption performance, including extraction time, ionic strength, and the type and volume of the desorption solvent. The method achieved limits of detection of 1 ng mL−1 and 3 ng mL−1 and quantification limits of 4 ng mL−1 and 10 ng mL−1 for lorazepam and diazepam, respectively. Furthermore, the developed method demonstrated good repeatability with relative standard deviations of 4% and 6% (n = 5) for the spiked analyte aqueous solutions at 50 ng mL−1. The method also exhibited high linearity (R > 0.9996) in the range from 10 to 1000 ng mL−1. [ABSTRACT FROM AUTHOR]

We measured the intracellular concentrations of tenofovir-diphosphate (TFV-DP) and emtricitabine-triphosphate (FTC-TP) in dried blood spots (DBS) for pre-exposure prophylaxis (PrEP) adherence using sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS). A total of 191 DBS were obtained from 85 participants who were receiving tenofovir disoproxil fumarate (TDF; 300 mg) and emtricitabine (FTC; 200 mg) as PrEP at the Sexual Health Clinic, National Center for Global Health and Medicine, Tokyo, Japan. DBS punch (3 mm) added to 25 μL of 50% methanol and 400 μL of internal standard solution was used for solid phase extraction. Chromatographic separation was achieved on an Atlantis Premier BEH C18 AX Column (50 mm × 2.1 mm i.d.; particle size 1.7 μm) using gradient elution (flow rate: 0.6 mL/min); injection volume: 7 μL and run time: 5.5 min. Calibration curves for the two drugs were linear in the range 0.05–12.5 ng/punch. We determined the intracellular TFV-DP and FTC-TP concentrations in 191 DBS obtained from 85 patients administered with TDF and FTC as PrEP. The analytical performance data (calibration curve and QC samples) for all the analytical runs met the acceptance criteria. Intracellular concentrations of TFV-DP and FTC-TP in the DBS remained stable for at least 24 h after oral administration. A multiplex LC–MS/MS method was successfully developed for DBS, which can be useful for monitoring the levels of TFV-DP and FTC-TP in individuals receiving PrEP. [ABSTRACT FROM AUTHOR]

The three-dimensional imprinted polymeric network was synthesized via a bulk polymerization reaction in the presence of a flavonoid as a template. In this reaction, methacrylic acid (MAA) and acrylic acid (AA), tetrahydrofuran and trimethylolpropanetrimethacrylate, were used as functional monomers, porogen, and cross-linker, respectively. In this study, two kinds of molecularly imprinted polymers (MIPs) with different ratios of 1:8:40 and 1:20:80 (template: functional monomer: cross-linker) were synthesized and compared together. The related binding capacities were calculated as equal to 392.08 mg/g and 609.00 mg/g, respectively, by UV-spectrometer. The synthesized polymers have been evaluated via field emission scan electron microscopy, transmission electron microscopy, and Brunauer–Emmett–Teller techniques. High selectivity and the proper specific surface area as equal to 167.00 m2/g in MIPs-based methacrylic acid (MIPs-MAA) and 434 m2/g in MIPs-based acrylic acid (MIPs-AA) comparatively to non-imprinted molecular polymers are the privileged characteristics in this research. The MIPs provided are a good candidate for the separation of flavonoids with the solid phase extraction method. [ABSTRACT FROM AUTHOR]

This study introduces a miniaturised solid-phase extraction (µ-SPE) method coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous quantification of 23 compounds, including psychoactive drugs, narcotics and their metabolites, in urine samples. The µ-SPE method, using standard laboratory equipment such as a centrifuge, was developed and validated, offering a practical and economical alternative to more traditional SPE methods. The key extraction parameters: elution solvent composition, sample and elution volumes, and sorbent mass were optimized to enhance performance. The method demonstrated high sensitivity, with detection limits between 0.06 and 0.41 ng cm−3 and quantification limits from 0.19 to 1.24 ng cm−3. The precision was confirmed with an intra-day precision ranging from 0.2% to 7.5% and an inter-day precision from 1.2% to 13.4%. Recovery rates ranged from 84.2% to 109.4%, with minimal matrix effects observed for most analytes (|ME|< 10%). The relative error remained below 5%, indicating good accuracy. The method was also evaluated in terms of greenness, practical, and analytical aspects using the WAC model. Based on the validation results, it was concluded that the developed method could be a good confirmatory method for results obtained by immunochemical tests and could also be used in both clinical analyses and forensic toxicology. [ABSTRACT FROM AUTHOR]

A novel magnetic molecular-imprinted polymer (MMIP) was used to selectively extract folic acid directly from real samples. Folic acid was used as template molecule, Fe3O4/SiO2-3-triethoxysilyl-propyl-acrylamide as functional monomer, azobisisobutyronitrile as initiation, ethylene glycol dimethacrylate as crosslinker agent, and acrylamide as the secondary monomer in a mixed ethanol-water solvent. The effect of different parameters on the extraction efficiency was studied, and the optimum conditions were established as follows: the concentrations of crosslinking and template were fixed at 0.05 and 0.06 g, absorption percentage was 96.5, pH was adjusted to 8, and extraction time was 8 h with a temperature of 25 °C. By examining the effect of pH, we tried to investigate the effect of the amide groups that present in MMIP and its intermolecular hydrogen interaction with folic acid. After optimising the effective parameters in polymer synthesis and adsorption rate, a magnetic imprinting dispersive solid-phase extraction method combined with fluorescence spectrophotometry at λem = 367 nm (MMIP-DSPE-FL) was constructed for sensitive determination of folic acid in tomato samples. The limit of quantification (LOQ) and limit of detection (LOD) values were 30.00 ± 0.01 μg L−1 and 10.00 ± 0.03 μg L−1, respectively, after the MMIP-DSPE preconcentration. Three tomato samples were analysed to give recoveries in the range of 80.2–81.6%, with relative standard deviation values below 0.6% (n = 3). The prepared MMIP-DSPE showed high selectivity toward folic acid, which could be used six times without changing adsorption capacity. The adsorption isotherm of the folic acid-imprinted polymer pursued the Langmuir model (RL = 0.029), and the kinetics model followed pseudo-first-order (R 2 = 0.9974). [ABSTRACT FROM AUTHOR]

Copyright of Journal of Chinese Institute of Food Science & Technology / Zhongguo Shipin Xuebao is the property of Journal of Chinese Institute of Food Science & Technology Periodical Office and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Copyright of Journal of Chinese Institute of Food Science & Technology / Zhongguo Shipin Xuebao is the property of Journal of Chinese Institute of Food Science & Technology Periodical Office and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test. [ABSTRACT FROM AUTHOR]